CN115096964A - Electrochemical sensor based on MXene porous structure and preparation method and application thereof - Google Patents
Electrochemical sensor based on MXene porous structure and preparation method and application thereof Download PDFInfo
- Publication number
- CN115096964A CN115096964A CN202210887858.9A CN202210887858A CN115096964A CN 115096964 A CN115096964 A CN 115096964A CN 202210887858 A CN202210887858 A CN 202210887858A CN 115096964 A CN115096964 A CN 115096964A
- Authority
- CN
- China
- Prior art keywords
- mxene
- electrochemical sensor
- porous structure
- prepare
- sensor based
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 43
- 239000004094 surface-active agent Substances 0.000 claims abstract description 25
- 239000011521 glass Substances 0.000 claims abstract description 19
- 239000003960 organic solvent Substances 0.000 claims abstract description 14
- 150000001875 compounds Chemical class 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000011148 porous material Substances 0.000 claims description 26
- 239000000243 solution Substances 0.000 claims description 26
- 238000001514 detection method Methods 0.000 claims description 23
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 18
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical group ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 12
- 238000005266 casting Methods 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 239000000758 substrate Substances 0.000 claims description 8
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 claims description 6
- 239000012528 membrane Substances 0.000 claims description 4
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- XRWMGCFJVKDVMD-UHFFFAOYSA-M didodecyl(dimethyl)azanium;bromide Chemical group [Br-].CCCCCCCCCCCC[N+](C)(C)CCCCCCCCCCCC XRWMGCFJVKDVMD-UHFFFAOYSA-M 0.000 claims description 3
- PSLWZOIUBRXAQW-UHFFFAOYSA-M dimethyl(dioctadecyl)azanium;bromide Chemical compound [Br-].CCCCCCCCCCCCCCCCCC[N+](C)(C)CCCCCCCCCCCCCCCCCC PSLWZOIUBRXAQW-UHFFFAOYSA-M 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- VIXPKJNAOIWFMW-UHFFFAOYSA-M dihexadecyl(dimethyl)azanium;bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)CCCCCCCCCCCCCCCC VIXPKJNAOIWFMW-UHFFFAOYSA-M 0.000 claims description 2
- IRMGVPILCPGYNQ-UHFFFAOYSA-M dimethyl-di(tetradecyl)azanium;bromide Chemical compound [Br-].CCCCCCCCCCCCCC[N+](C)(C)CCCCCCCCCCCCCC IRMGVPILCPGYNQ-UHFFFAOYSA-M 0.000 claims description 2
- 238000012856 packing Methods 0.000 claims description 2
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 abstract description 72
- 229960003638 dopamine Drugs 0.000 abstract description 36
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 230000035945 sensitivity Effects 0.000 description 19
- 239000000463 material Substances 0.000 description 18
- 239000002131 composite material Substances 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 230000004043 responsiveness Effects 0.000 description 7
- 238000010276 construction Methods 0.000 description 6
- 230000002829 reductive effect Effects 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000012074 organic phase Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 230000029058 respiratory gaseous exchange Effects 0.000 description 4
- 230000004044 response Effects 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000004964 aerogel Substances 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 238000004220 aggregation Methods 0.000 description 3
- 238000001338 self-assembly Methods 0.000 description 3
- 230000003068 static effect Effects 0.000 description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000000835 electrochemical detection Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000002452 interceptive effect Effects 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 230000000670 limiting effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- LEHOTFFKMJEONL-UHFFFAOYSA-N Uric Acid Chemical compound N1C(=O)NC(=O)C2=C1NC(=O)N2 LEHOTFFKMJEONL-UHFFFAOYSA-N 0.000 description 1
- TVWHNULVHGKJHS-UHFFFAOYSA-N Uric acid Natural products N1C(=O)NC(=O)C2NC(=O)NC21 TVWHNULVHGKJHS-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- QGJOPFRUJISHPQ-NJFSPNSNSA-N carbon disulfide-14c Chemical compound S=[14C]=S QGJOPFRUJISHPQ-NJFSPNSNSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 235000001727 glucose Nutrition 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000007641 inkjet printing Methods 0.000 description 1
- 239000000138 intercalating agent Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 230000001404 mediated effect Effects 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 238000006486 pseudo-catalysis Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- -1 transition metal carbides Chemical class 0.000 description 1
- 229940116269 uric acid Drugs 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Molecular Biology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
The invention discloses an electrochemical sensor based on an MXene porous structure, and a preparation method and application thereof, and belongs to the technical field of electrochemical sensing. The method comprises the steps of coating MXene by using a surfactant to prepare an MXene-based compound, dissolving the compound in an organic solvent to prepare an organic solution containing MXene at a certain concentration, pouring the prepared MXene-based organic solution on ITO conductive glass under a high humidity condition, and forming an MXene-based porous film on the ITO conductive glass after the organic solvent and water are completely volatilized, namely the electrochemical sensor based on an MXene porous structure can be used for detecting dopamine. The invention provides the electrochemical sensor which is low in cost, simple, convenient, green, environment-friendly, easy to carry, easy to operate and sensitive and can be used for detecting dopamine.
Description
Technical Field
The invention relates to the technical field of electrochemical sensing, in particular to an electrochemical sensor based on an MXene porous structure and a preparation method and application thereof.
Background
Two-dimensional materials have attracted much attention due to their excellent chemical and physical properties, and a new class of two-dimensional transition metal carbides, nitrides and carbonitrides, namely MXene, has become a recent research focus due to its unique two-dimensional layered structure and various properties imparted by functional groups, such as good electrical conductivity, surface hydrophilicity and mechanical properties. However, similar to other two-dimensional materials, aggregation between adjacent MXene sheets is easily caused by van der waals force and hydrogen bonding, which results in reduction of surface active area and deterioration of electrical conductivity, etc., thereby affecting various properties. In order to fully utilize the electrochemical properties of MXene nanosheets, various methods for inhibiting aggregation of the lamellae thereof have been developed, such as the introduction of an intercalating agent, the construction of a three-dimensional structure, and the like. Wherein the construction of three-dimensional porous structure is an effective means. On one hand, the excellent characteristics of MXene can be converted from nanometer scale to macroscopic scale through the construction of the three-dimensional porous structure, and on the other hand, the construction of the three-dimensional porous structure may introduce other characteristics beneficial to practical application. MXene-based porous gels can be prepared, for example, by combining 3D ink jet printing with unidirectional freeze casting, which have excellent electromechanical and electrochemical properties [3D printed MXene aerogels with a pipeline 3D macroscopic structure and a high engineered microscopic structure for enhanced electrical and electrochemical performance [ J ]. Advanced Materials, 2022, 34: 2104980 ]. By introducing KOH during the self-assembly process, Porous MXene materials can be prepared that have good rate capability and enhanced electrochemical properties such as reversible high capacity [ Porous MXene monomers with localized chemistry-mediated structure for enhanced pseudo-catalysis and fast sodium-ion storage [ J ]. Nano Energy, 2021, 86: 106091 ]. In addition, through the construction of porous structures, MXene and rGO hybrid aerogel-based piezoresistive sensors show better performance than either single pure component [3D synthetic MXene/reduced graphene oxide aerogel for a piezoreactive sensor [ J ]. ACS Nano, 2018, 12: 3209-. The results prove that the construction of the three-dimensional porous structure has a beneficial effect on the aspect of improving the electrochemical performance of the MXene-based material.
Accordingly, researchers have developed various methods for preparing MXene-based porous structures, such as sacrificial templating, gelation, lyophilization, and loading on three-dimensional substrates. However, these methods may involve the use of toxic reagents such as hydrazine hydrate, complicated procedures, high temperature calcination processes that can accelerate MXene oxidation, and the like. Therefore, if a simple, non-toxic and mild method for preparing the MXene-based porous structure can be developed and the MXene-based porous structure is used as an electrochemical sensor, the method plays an important role in improving the performance of the sensor and realizing practical application.
Disclosure of Invention
The invention aims to provide an electrochemical sensor based on an MXene porous structure and a preparation method and application thereof, and aims to solve the problems that MXene in an MXene base material is easy to aggregate, steps in the preparation methods of the MXene porous material and the MXene porous material based electrochemical sensor are complex, toxic substances are used, the porous structure and the electrochemical performance are difficult to regulate and the like in the prior art.
The MXene-based composite is prepared by selecting a proper amount of the surfactant, a proper amount of the MXene, a proper ratio of the surfactant to the MXene and a simple self-assembly process, transferring the MXene from a water phase to an organic phase, and preparing the MXene-based composite by selecting the proper amount of the composite, the pouring amount of an organic solution of the composite, the humidity and other conditions, taking ITO conductive glass as a substrate, and using a static breathing pattern method and water drops as a pore-forming template to prepare the MXene-based porous membrane attached to the ITO conductive glass, namely the electrochemical sensor based on the MXene porous structure, which can be used for detecting biomolecules such as dopamine.
In order to achieve the above purpose, the invention provides the following scheme: the invention provides an electrochemical sensor based on an MXene porous structure, which comprises an ITO conductive glass substrate and an MXene porous film attached to the ITO conductive glass substrate, wherein holes in the MXene porous film are in honeycomb hexagonal stacking arrangement and are uniform in size, and the average pore diameter is 1.2-15.0 microns. The electrochemical sensor can be used for electrochemical detection of dopamine, and has the advantages of high sensitivity, low detection limit, good anti-interference performance, repeatability and stability.
The invention also provides a preparation method of the electrochemical sensor based on the MXene porous structure, which comprises the following steps:
(1) dispersing MXene in deionized water to prepare an MXene aqueous solution;
(2) dissolving a surfactant in an organic solvent to prepare a surfactant organic solution;
(3) mixing the MXene aqueous solution prepared in the step (1) and the surfactant organic solution prepared in the step (2) according to a certain proportion, and stirring to prepare an MXene-based compound;
(4) dissolving the MXene-based compound prepared in the step (3) in an organic solvent to prepare an MXene compound organic solution;
(5) and (5) pouring the MXene compound organic solution prepared in the step (4) with a certain volume on ITO conductive glass under high humidity to prepare ITO glass loaded with the MXene-based porous film, namely the electrochemical sensor based on the MXene porous structure.
In a further preferred embodiment of the present invention, the concentration of MXene in step (1) is 0.1 to 5.0 mg/mL.
Further preferably, in the step (2), the concentration of the surfactant is 0.03-1.50 mg/mL; the surfactant is didodecyl dimethyl ammonium bromide, ditetradecyl dimethyl ammonium bromide, dihexadecyl dimethyl ammonium bromide, dioctadecyl dimethyl ammonium bromide and hexadecyl trimethyl ammonium bromide; the organic solvent is chloroform and dichloromethane.
In a further preferable aspect of the present invention, the volume ratio of the MXene aqueous solution to the surfactant organic solution in the step (3) is 1:1 to 1: 5.
According to further optimization of the invention, the concentration of the MXene-based compound in the step (4) is 1-3 mg/mL; the organic solvent is dichloromethane, chloroform and carbon disulfide.
According to further optimization of the invention, the casting volume in the step (5) is 20-100 mu L; the humidity is 55-95%.
An application of an electrochemical sensor in the field of biomolecule detection.
The method selects proper MXene dosage and the type and dosage of the surfactant, prepares the MXene-based composite by a self-assembly process, selects proper MXene-based composite dosage, pours the MXene-based composite dosage on the ITO conductive glass under the high humidity condition, and prepares the MXene-based porous film loaded on the ITO conductive glass by a breathing pattern method. The MXene-based porous film can inhibit the overlapping and aggregation of MXene sheet layers, so that the contactable electrochemical active area of the MXene-based porous film is increased, and the electrochemical detection efficiency is improved. In addition, the MXene-based porous structure is constructed by adopting a static breathing pattern method, volatile water drops are taken as a template of the porous structure, the method has the advantages of simplicity, convenience, environmental friendliness, low cost and the like, and moreover, the preparation of the electrochemical sensor based on the MXene porous structure is realized while the MXene-based porous structure is formed by taking ITO conductive glass as a casting film substrate, so that the preparation process of the electrochemical sensor is simplified, the preparation cost is reduced, and the green preparation of the electrochemical sensor is realized.
The invention discloses the following technical effects:
the invention discloses an electrochemical sensor based on an MXene porous structure and a preparation method thereof, wherein the electrochemical sensor comprises the following steps: the electrochemical sensor comprises an ITO glass substrate and an MXene-based porous membrane attached to the ITO glass substrate, holes in the porous membrane are arranged in a honeycomb hexagonal stacking mode, the pore size is uniform, and the average size of the pore size is about 1.2-15.0 microns. When the electrochemical sensor is used for detecting dopamine, the electrochemical sensor shows higher sensitivity, lower detection limit, better repeatability, anti-interference performance, stability and the like.
The MXene-based porous structure is prepared by using a simple, convenient and easy-to-operate static breathing pattern method, the method takes easily-obtained, cheap, volatile and removed water drops as a template of the porous structure, and has the advantages of simplicity, convenience, cheapness, environmental friendliness and the like.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
Fig. 1 is a scanning electron microscope picture of a porous structure in the electrochemical sensor based on an MXene porous structure prepared in example 1.
Fig. 2 shows DPV data of electrochemical sensors based on MXene porous structure prepared in example 1 for detecting different concentrations of dopamine.
Fig. 3 is a graph showing the current response of the electrochemical sensor based on the MXene porous structure prepared in example 1 to dopamine and other interfering substances.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but rather as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The description and examples are intended to be illustrative only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including but not limited to.
Example 1
(1) 1mg MXene was dispersed in 1mL deionized water;
(2) 0.3mg dioctadecyldimethylammonium bromide is dispersed in 1mL chloroform;
(3) mixing the MXene aqueous solution prepared in the step (1) and the surfactant organic solution prepared in the step (2) according to the volume ratio of 1:1, and stirring to prepare an MXene-based compound;
(4) dissolving 2mg of the MXene-based complex prepared in the step (3) in 1mL of chloroform to prepare an MXene complex organic solution;
(5) and (5) pouring 50 mu L of the MXene compound organic solution prepared in the step (4) on ITO conductive glass at 75% humidity to prepare the ITO glass loaded with the MXene-based porous film, namely the electrochemical sensor based on the MXene porous structure.
Fig. 1 is a scanning electron microscope image of the porous structure of the electrochemical sensor based on the MXene porous structure obtained in this example, and it can be seen from fig. 1 that almost every hole in the porous structure is surrounded by other six holes, forming a hexagonal packing structure similar to a honeycomb, and the size of the hole is uniform, and the size of the hole is about 2.6 μm.
FIG. 2 is the DPV data of the electrochemical sensor based on the MXene porous structure for detecting dopamine with different concentrations, and it can be seen from FIG. 2 that the linear regression equation of the oxidation peak current and the dopamine concentration is I p =4.09804c–3.211595 (0μM~10μM,R 2 =0.994) and I p =1.19377c+29.92342 (10μM~50μM,R 2 =0.997), sensitivity is 4.098 μ a. μ M -1 •cm -2 The detection limit was 36.8nM (signal-to-noise ratio S/N = 3).
Fig. 3 shows the current response of the electrochemical sensor based on the MXene porous structure prepared in this embodiment to dopamine and other interfering substances, and as can be seen from fig. 3, the MXene porous film-based electrochemical sensor only responds to dopamine, but does not respond to other substances such as calcium chloride, sodium carbonate, magnesium chloride, sodium chloride, potassium chloride, uric acid, lactic acid, glucose, ascorbic acid, and the like, and shows better anti-interference performance.
The electrochemical sensor based on the MXene porous structure is subjected to 5 parallel dopamine response experiments, the relative standard deviation is only 0.74%, and good repeatability is proved. The response current of the electrochemical sensor to dopamine still keeps more than 92% of the initial current value after 9 days, and the electrochemical sensor is proved to have better stability.
Example 2
The above procedure was repeated to prepare an electrochemical sensor based on an MXene porous structure, with the same materials and conditions as in example 1, except that the amount of MXene was reduced to 0.1 mg. The pore size of the porous structure in the electrochemical sensor prepared in the embodiment is about 2 μ M, and the sensitivity for detecting dopamine is 0.98 μ A. μ M -1 •cm -2 The detection limit was 220.5nM (signal-to-noise ratio S/N = 3). And has good anti-interference performance, repeatability and stability.
Example 3
The same as example 1, except for increasing the amount of MXene to 5mg, the above procedure was repeated to prepare an electrochemical sensor based on MXene porous structure. The pore diameter of the porous structure in the electrochemical sensor prepared in the embodiment is about 14.5 μ M, and the sensitivity for detecting dopamine is 2.28 μ A. μ M -1 •cm -2 The detection limit was 120.5nM (signal-to-noise ratio S/N = 3). And has good anti-interference performance, repeatability and stability.
Example 4
The above procedure was repeated to prepare an electrochemical sensor based on an MXene porous structure, with the same materials and conditions as in example 1, except that the amount of the surfactant was reduced to 0.03 mg. The pore diameter of the porous structure in the electrochemical sensor prepared in the embodiment is about 14 μ M, and the sensitivity for detecting dopamine is 2.5 μ A. μ M -1 •cm -2 The detection limit was 115nM (signal-to-noise ratio S/N = 3). And has good anti-interference performance, repeatability and stability.
Example 5
The above procedure was repeated to prepare an electrochemical sensor based on an MXene porous structure, with the same substance and conditions as in example 1, except that the amount of the surfactant was increased to 1.5 mg. The pore diameter of the porous structure in the electrochemical sensor prepared in the embodiment is about 1.98 μ M, and the sensitivity for detecting dopamine is 1.38 μ A. mu.M -1 •cm -2 The detection limit was 210nM (signal-to-noise ratio S/N = 3). And has good anti-interference performance, repeatability and stability.
Example 6
The same as example 1, except for changing the surfactant to didodecyldimethylammonium bromide and repeating the above steps, an electrochemical sensor based on an MXene porous structure was prepared. The pore diameter of the porous structure in the electrochemical sensor prepared in the embodiment is about 2.5 μ M, and the sensitivity for detecting dopamine is 4 μ A. μ M -1 •cm -2 The detection limit was 50nM (signal-to-noise ratio S/N = 3). And has good anti-interference performance, repeatability and stability.
Example 7
The same as example 1, except for changing the surfactant to cetyltrimethylammonium bromide and repeating the above steps, an electrochemical sensor based on MXene porous structure was prepared. The pore diameter of the porous structure in the electrochemical sensor prepared in the embodiment is about 2.3 μ M, and the sensitivity for detecting dopamine is 3.9 μ A. μ M -1 •cm -2 The detection limit was 65nM (signal-to-noise ratio S/N = 3). And has good anti-interference performance, repeatability and stability.
Example 8
The same as example 1, except for changing the organic solvent in which the surfactant was dissolved to dichloromethane, the above procedure was repeated to prepare an electrochemical sensor based on an MXene porous structure. The pore diameter of the porous structure in the electrochemical sensor prepared in the embodiment is about 3.0 μ M, and the sensitivity for detecting dopamine is 3.35 μ A. μ M -1 •cm -2 The detection limit was 80nM (signal-to-noise ratio S/N = 3). And has good anti-interference performance, repeatability and stability.
Example 9
The same as example 1, except that the volume ratio of the aqueous MXene solution to the organic surfactant solution was changed to 1:5, the above steps were repeated to prepare an electrochemical sensor based on the porous MXene structure. The pore size of the porous structure in the electrochemical sensor manufactured in this example was about 1.8 μm,the sensitivity for detecting dopamine is 1.32 muA. mu.M -1 •cm -2 The detection limit was 218nM (signal-to-noise ratio S/N = 3). And has good anti-interference performance, repeatability and stability.
Example 10
The same as example 1, except that the amount of the MXene-based complex was increased to 3mg, the above procedure was repeated to prepare an electrochemical sensor based on the MXene porous structure. The pore diameter of the porous structure in the electrochemical sensor prepared in the embodiment is about 2.1 μ M, and the sensitivity for detecting dopamine is 4.05 μ A. μ M -1 •cm -2 The detection limit was 45.4nM (signal-to-noise ratio S/N = 3). And has good anti-interference performance, repeatability and stability.
Example 11
The above procedure was repeated to prepare an electrochemical sensor based on an MXene porous structure, as in example 1, except that the amount of the MXene-based complex was reduced to 1 mg. The pore size of the porous structure in the electrochemical sensor prepared in the embodiment is about 3.5 μ M, and the sensitivity for detecting dopamine is 3.92 μ A. μ M -1 •cm -2 The detection limit was 53nM (signal-to-noise ratio S/N = 3). And has good anti-interference performance, repeatability and stability.
Example 12
The same as example 1, except for changing the organic solvent for dissolving the composite into carbon disulfide, and repeating the above steps to prepare the electrochemical sensor based on the MXene porous structure. The pore size of the porous structure in the electrochemical sensor prepared in the embodiment is about 1.5 μ M, and the sensitivity for detecting dopamine is 4.05 μ A. μ M -1 •cm -2 The detection limit was 40nM (signal-to-noise ratio S/N = 3). And has good anti-interference performance, repeatability and stability.
Example 13
The same as example 1, except for changing the organic solvent for dissolving the complex to dichloromethane, the above procedure was repeated to prepare an electrochemical sensor based on an MXene porous structure. The electrochemical sensor prepared in this example had a porous structureThe pore diameter is about 2.3 mu M, and the sensitivity for detecting dopamine is 3.95 mu A. mu.M -1 •cm -2 The detection limit was 54.5nM (signal-to-noise ratio S/N = 3). And has good anti-interference performance, repeatability and stability.
Example 14
The electrochemical sensor based on MXene porous structure was prepared by repeating the above steps with the casting volume of the composite organic solution changed to 20. mu.L as in example 1 except that the other materials and conditions were not changed. The pore diameter of the porous structure in the electrochemical sensor prepared in the embodiment is about 2.05 μ M, and the sensitivity for detecting dopamine is 4.02 μ A. μ M -1 •cm -2 The detection limit was 38.5nM (signal-to-noise ratio S/N = 3). And has good anti-interference performance, repeatability and stability.
Example 15
The electrochemical sensor based on the MXene porous structure is prepared by repeating the steps as same as example 1, except that the casting volume of the composite organic solution is changed to 100 μ L. The pore size of the porous structure in the electrochemical sensor prepared in the embodiment is about 2.09 μ M, and the sensitivity for detecting dopamine is 3.99 μ A. μ M -1 •cm -2 The detection limit was 51.2nM (signal-to-noise ratio S/N = 3). And has good anti-interference performance, repeatability and stability.
Example 16
The same as example 1, except that the casting humidity of the composite organic solution was changed to 55%, the above steps were repeated to prepare an electrochemical sensor based on an MXene porous structure. The pore diameter of the porous structure in the electrochemical sensor prepared in the embodiment is about 1.2 μ M, and the sensitivity for detecting dopamine is 2.35 μ A. μ M -1 •cm -2 The detection limit was 119.7nM (signal-to-noise ratio S/N = 3). And has good anti-interference performance, repeatability and stability.
Example 17
The same as example 1, except that the casting humidity of the composite organic solution was changed to 95%, the above steps were repeated to prepare an electrochemical sensor based on an MXene porous structure. Book (I)The electrochemical sensor prepared in the example has a porous structure with a pore size of about 15 μ M and a dopamine detection sensitivity of 0.8 μ A. μ M -1 •cm -2 The detection limit was 270.8nM (signal-to-noise ratio S/N = 3). And has good anti-interference performance, repeatability and stability.
Comparative example 1
The electrochemical sensor was prepared by repeating the above steps while changing the casting humidity of the composite organic solution to 40% as in example 1, except that other materials and conditions were not changed. The electrochemical sensor prepared by the embodiment has almost no porous structure, and has poor electrochemical responsiveness when detecting dopamine.
Comparative example 2
The electrochemical sensor based on MXene porous structure was prepared by repeating the above steps with the casting volume of the composite organic solution changed to 5. mu.L as in example 1 except that the other materials and conditions were not changed. The electrochemical sensor prepared by the embodiment has poor coverage of the porous structure on the ITO glass, poor uniformity and orderliness of the porous structure, and poor electrochemical responsiveness in dopamine detection.
Comparative example 3
The same as example 1, except for changing the organic solvent for dissolving the complex to toluene, the above procedure was repeated to prepare an electrochemical sensor based on an MXene porous structure. The electrochemical sensor prepared by the embodiment has poor uniformity and orderliness of a porous structure, and has poor electrochemical responsiveness when detecting dopamine.
Comparative example 4
The procedure of example 1 was repeated except that the amount of MXene-based complex was reduced to 0.05mg, and other materials and conditions were changed to prepare an electrochemical sensor. The electrochemical sensor prepared by the embodiment has almost no porous structure, and has poor electrochemical responsiveness when detecting dopamine.
Comparative example 5
The same as example 1, except for changing the volume ratio of the MXene aqueous solution to the surfactant organic solution to 1:20, the other materials and conditions were changed, and the above-described procedure was repeated to prepare an electrochemical sensor. In the process of preparing the electrochemical sensor, the effect of transferring MXene from a water phase to an organic phase is poor, the pore diameter of the porous structure in the prepared electrochemical sensor is not uniform, the arrangement is disordered, and the electrochemical responsiveness is poor when dopamine is detected.
Comparative example 6
The same as example 1, except for increasing the amount of the surfactant to 5mg, other materials and conditions were unchanged, and the above procedure was repeated to prepare an electrochemical sensor. In the process of preparing the electrochemical sensor, the effect of transferring MXene from a water phase to an organic phase is poor, the pore diameter of the porous structure in the prepared electrochemical sensor is not uniform, the arrangement is disordered, and the electrochemical responsiveness is poor when dopamine is detected.
Comparative example 7
The same as example 1, except for increasing the amount of MXene to 10mg, the other materials and conditions were changed, and the above-described procedure was repeated to prepare an electrochemical sensor. In the process of preparing the electrochemical sensor, the effect of transferring MXene from a water phase to an organic phase is poor, the pore diameter of the porous structure in the prepared electrochemical sensor is not uniform, the arrangement is disordered, and the electrochemical responsiveness is poor when dopamine is detected.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (9)
1. An electrochemical sensor based on an MXene porous structure is characterized by comprising an ITO glass substrate and an MXene-based honeycomb porous membrane.
2. The electrochemical sensor as claimed in claim 1, wherein the MXene-based porous structure has pores in hexagonal packing arrangement similar to honeycomb shape, uniform size, and average pore diameter of about 1.2-15.0 μm.
3. A method for preparing an electrochemical sensor based on an MXene porous structure of claim 1 or 2, comprising the steps of:
(1) dispersing MXene in deionized water to prepare an MXene aqueous solution;
(2) dissolving a surfactant in an organic solvent to prepare a surfactant organic solution;
(3) mixing the MXene aqueous solution prepared in the step (1) and the surfactant organic solution prepared in the step (2) according to a certain proportion, and stirring to prepare an MXene-based compound;
(4) dissolving the MXene-based compound prepared in the step (3) in an organic solvent to prepare an MXene compound organic solution;
(5) pouring a certain volume of the MXene compound organic solution prepared in the step (4) on ITO conductive glass under high humidity to prepare ITO glass loaded with the MXene-based porous film, namely the electrochemical sensor based on the MXene porous structure.
4. The method as claimed in claim 3, wherein the concentration of MXene in step (1) is 0.1-5.0 mg/mL.
5. The method for preparing the electrochemical sensor based on the MXene porous structure according to claim 3, wherein the surfactant concentration in the step (2) is 0.03-1.50 mg/mL; the surfactant is didodecyldimethylammonium bromide, ditetradecyldimethylammonium bromide, dihexadecyldimethylammonium bromide, dioctadecyldimethylammonium bromide and hexadecyltrimethylammonium bromide; the organic solvent is chloroform and dichloromethane.
6. The method for preparing the electrochemical sensor based on the MXene porous structure, according to claim 3, wherein the volume ratio of the MXene aqueous solution to the surfactant organic solution in the step (3) is 1: 1-1: 5.
7. The method for preparing the electrochemical sensor based on the MXene porous structure according to claim 3, wherein the concentration of the MXene-based complex in the step (4) is 1-3 mg/mL; the organic solvent is dichloromethane, chloroform and carbon disulfide.
8. The method for preparing the electrochemical sensor based on the MXene porous structure, characterized in that in the step (5), the casting volume is 20-100 μ L; the humidity is 55-95%.
9. Use of an electrochemical sensor according to claim 1 or 2 in the field of biomolecule detection.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202210887858.9A CN115096964B (en) | 2022-07-26 | 2022-07-26 | Electrochemical sensor based on MXene porous structure and preparation method and application thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202210887858.9A CN115096964B (en) | 2022-07-26 | 2022-07-26 | Electrochemical sensor based on MXene porous structure and preparation method and application thereof |
Publications (2)
Publication Number | Publication Date |
---|---|
CN115096964A true CN115096964A (en) | 2022-09-23 |
CN115096964B CN115096964B (en) | 2024-04-05 |
Family
ID=83297976
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202210887858.9A Active CN115096964B (en) | 2022-07-26 | 2022-07-26 | Electrochemical sensor based on MXene porous structure and preparation method and application thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN115096964B (en) |
Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR20170106857A (en) * | 2016-03-14 | 2017-09-22 | 한국에너지기술연구원 | Preparing method of the 3D porous structured graphene/Mxene composite by ice-templating method and 3D porous structured graphene/Mxene composite by the same method |
CN108329689A (en) * | 2018-03-08 | 2018-07-27 | 哈尔滨理工大学 | A kind of low dielectric coefficient polyimide porous membrane and preparation method thereof |
CN110589786A (en) * | 2019-10-16 | 2019-12-20 | 大连理工大学 | Based on three-dimensional porous transition metal carbide Ti3C2MXene composite nano structure and general preparation method thereof |
CN111087634A (en) * | 2019-12-17 | 2020-05-01 | 广东省石油与精细化工研究院 | Nano-composite porous polyimide film and preparation method thereof |
CN113041855A (en) * | 2021-03-23 | 2021-06-29 | 南京工业大学 | Two-dimensional porous MXene film and preparation method and application thereof |
CN113285070A (en) * | 2021-04-30 | 2021-08-20 | 天津大学 | Preparation method and application of MXene dense porous membrane with adjustable pores |
CN113777144A (en) * | 2021-11-09 | 2021-12-10 | 中国民航大学 | Electrochemical sensor for detecting dopamine in gastric juice and preparation method and application thereof |
-
2022
- 2022-07-26 CN CN202210887858.9A patent/CN115096964B/en active Active
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR20170106857A (en) * | 2016-03-14 | 2017-09-22 | 한국에너지기술연구원 | Preparing method of the 3D porous structured graphene/Mxene composite by ice-templating method and 3D porous structured graphene/Mxene composite by the same method |
CN108329689A (en) * | 2018-03-08 | 2018-07-27 | 哈尔滨理工大学 | A kind of low dielectric coefficient polyimide porous membrane and preparation method thereof |
CN110589786A (en) * | 2019-10-16 | 2019-12-20 | 大连理工大学 | Based on three-dimensional porous transition metal carbide Ti3C2MXene composite nano structure and general preparation method thereof |
CN111087634A (en) * | 2019-12-17 | 2020-05-01 | 广东省石油与精细化工研究院 | Nano-composite porous polyimide film and preparation method thereof |
CN113041855A (en) * | 2021-03-23 | 2021-06-29 | 南京工业大学 | Two-dimensional porous MXene film and preparation method and application thereof |
CN113285070A (en) * | 2021-04-30 | 2021-08-20 | 天津大学 | Preparation method and application of MXene dense porous membrane with adjustable pores |
CN113777144A (en) * | 2021-11-09 | 2021-12-10 | 中国民航大学 | Electrochemical sensor for detecting dopamine in gastric juice and preparation method and application thereof |
Non-Patent Citations (1)
Title |
---|
JUNMING ZHANG 等: "3D porous structure assembled from MXene via breath figure method for electrochemical detection of dopamine", CHEMICAL ENGINEERING JOURNAL, vol. 452, pages 139414 * |
Also Published As
Publication number | Publication date |
---|---|
CN115096964B (en) | 2024-04-05 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Qiu et al. | Recent advance in fabricating monolithic 3D porous graphene and their applications in biosensing and biofuel cells | |
Shi et al. | High-performance capacitive deionization via manganese oxide-coated, vertically aligned carbon nanotubes | |
Zhang et al. | Electrospinning design of functional nanostructures for biosensor applications | |
Zhang et al. | Nanoparticles-assembled NiO nanosheets templated by graphene oxide film for highly sensitive non-enzymatic glucose sensing | |
Tomer et al. | Cubic mesoporous Ag@ CN: a high performance humidity sensor | |
Yang et al. | A novel quercetin electrochemical sensor based on molecularly imprinted poly (para-aminobenzoic acid) on 3D Pd nanoparticles-porous graphene-carbon nanotubes composite | |
US10258932B2 (en) | Porous carbon films | |
Huang et al. | Large-scale synthesis of hydrated tungsten oxide 3D architectures by a simple chemical solution route and their gas-sensing properties | |
Chen et al. | 3D porous and redox-active prussian blue-in-graphene aerogels for highly efficient electrochemical detection of H 2 O 2 | |
Liu et al. | Sulfur–nitrogen co-doped three-dimensional carbon foams with hierarchical pore structures as efficient metal-free electrocatalysts for oxygen reduction reactions | |
JP6305349B2 (en) | Highly sintered stable metal nanoparticles supported on mesoporous graphite particles and uses thereof | |
Ding et al. | Preparation of TiO 2–Pt hybrid nanofibers and their application for sensitive hydrazine detection | |
Brunet et al. | Properties of membranes containing semi-dispersed carbon nanotubes | |
Colomer et al. | High porosity silica xerogels prepared by a particulate sol–gel route: pore structure and proton conductivity | |
Yang et al. | Biomass-derived hierarchically porous CoFe-LDH/CeO2hybrid with peroxidase-like activity for colorimetric sensing of H2O2 and glucose | |
Guo et al. | Atomically thin SiC nanoparticles obtained via ultrasonic treatment to realize enhanced catalytic activity for the oxygen reduction reaction in both alkaline and acidic media | |
CN105129927B (en) | The preparation method of graphene/carbon nano-tube aeroge composite capacitance-type desalting electrode | |
Han et al. | Controlled synthesis of double-shelled CeO 2 hollow spheres and enzyme-free electrochemical bio-sensing properties for uric acid | |
Xu et al. | Fabrication of NiCo 2 O 4 and carbon nanotube nanocomposite films as a high-performance flexible electrode of supercapacitors | |
CN107703196B (en) | Preparation method of graphene-filter paper and application of graphene-filter paper as self-supporting flexible electrode | |
Chen et al. | Recent trends in synthesis and applications of porous MXene assemblies: A topical review | |
Ahmadi et al. | Synthesis of silver nano catalyst by gel-casting using response surface methodology | |
Yan et al. | Synthesis of 3D mesoporous samarium oxide hydrangea microspheres for enzyme-free sensor of hydrogen peroxide | |
CN107583662A (en) | A kind of oxygen reduction catalyst and its preparation method and application | |
KR20140104019A (en) | Process for preparing a sol-gel from at least three metal salts and use of the process for preparing a ceramic membrane |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |